CN104292495A - Preparation method of polystyrene foam microsphere - Google Patents
Preparation method of polystyrene foam microsphere Download PDFInfo
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- CN104292495A CN104292495A CN201410533506.9A CN201410533506A CN104292495A CN 104292495 A CN104292495 A CN 104292495A CN 201410533506 A CN201410533506 A CN 201410533506A CN 104292495 A CN104292495 A CN 104292495A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000004005 microsphere Substances 0.000 title abstract 4
- 229920006327 polystyrene foam Polymers 0.000 title abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000004793 Polystyrene Substances 0.000 claims abstract description 54
- 229920002223 polystyrene Polymers 0.000 claims abstract description 54
- 239000006260 foam Substances 0.000 claims abstract description 39
- 239000002131 composite material Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000008346 aqueous phase Substances 0.000 claims description 109
- 239000012071 phase Substances 0.000 claims description 85
- 239000000243 solution Substances 0.000 claims description 58
- 239000012153 distilled water Substances 0.000 claims description 53
- 239000008267 milk Substances 0.000 claims description 21
- 210000004080 milk Anatomy 0.000 claims description 21
- 235000013336 milk Nutrition 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000000520 microinjection Methods 0.000 claims description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 238000007711 solidification Methods 0.000 claims description 11
- 230000008023 solidification Effects 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000011010 flushing procedure Methods 0.000 claims description 10
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 10
- 238000004513 sizing Methods 0.000 claims description 10
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 8
- -1 filter Substances 0.000 claims description 7
- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 claims description 4
- 229920002125 Sokalan® Polymers 0.000 claims description 4
- 239000004584 polyacrylic acid Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 abstract 1
- 239000013557 residual solvent Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 238000004377 microelectronic Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000010094 polymer processing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000008259 solid foam Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Medicinal Preparation (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention provides a preparation method of a polystyrene foam microsphere. The preparation method mainly comprises the steps of: by virtue of manners of introducing a pore-forming agent into a polystyrene solution and introducing microbubbles through ultrasonic oscillation, preparing water-in-polystyrene-solution composite emulsifiable particles or polystyrene solid emulsifiable particles by virtue of a microfluidic technology, removing an organic solvent for dissolving a polystyrene-based polymer by virtue of a spin evaporation method and drying to remove water and residual solvent, thereby obtaining the polystyrene foam microsphere with narrow particle size distribution. The foam microsphere can be widely applied in the fields such as chemical catalysis and high-energy physical experiments.
Description
Technical field
The present invention relates to a kind of preparation method of polystyrene type foam microshell, belong to polymer processing forming field.Prepared preparation polystyrene type foam microshell can be widely used in the aspects such as biomedical diagnostic, microelectronics, chemical catalysis, high-energy physics experiment and Colloidal crystals template.
Background technology
Polystyrene type foam microshell, because having bigger serface, the strong advantage such as adsorptivity and solvent resistance, is widely used in the fields such as biomedical diagnostic, microelectronics, chemical catalysis and high-energy physics experiment.At present, the preparation of polystyrene type foam microshell adopts synthetic route usually, namely utilizes styrene monomer, initiator and dispersion agent etc., prepares polystyrene type foam microshell by the polyreaction such as emulsion or suspension polymerization.Preparation technology's more complicated of these polystyrene type foam microshells, complex operation, process is wayward.
Summary of the invention
The object of the invention is the preparation method providing a kind of polystyrene type foam microshell.
The preparation method of polystyrene type foam microshell of the present invention comprises the following steps successively:
A. polystyrenic polymer and pore-creating agent are dissolved in organic solvent, as oil phase;
B. newborn grain stablizer is dissolved in distilled water, filter, filtrate is as outer aqueous phase;
C. before newborn grain preparation, oil-phase solution is ultrasonic, a certain amount of distilled water, oil-phase solution and outer aqueous phase solution is drawn respectively with syringe, syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump;
D. regulate the flow velocity of micro-injection pump, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase;
E. collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 20
oc ~ 65
oc, speed of rotation 25 rpm ~ 65 rpm, set time 48 h ~ 96 h;
F. after solidification terminates, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains polystyrene type hollow foam microballoon.
When not introducing distilled water as interior aqueous phase, when only adopting oil phase and outer aqueous phase solution to prepare solid newborn grain, after solidification is dry, obtain polystyrene solid foam microballoon.
Polystyrenic polymer in step a mass percent in oil phase is 4.0% ~ 25.0%; Pore-creating agent mass percent in oil phase is 1.0% ~ 10%; Newborn grain stablizer in step b outside in aqueous phase mass percent be 0.01% ~ 4.0%.
In step a, polystyrenic polymer is polystyrene or perduterated polystyrene.
In step a, pore-creating agent is the one in hexane, dodecane, n-Hexadecane.
In step b, newborn grain stablizer comprises the one in polyoxyethylene, polyacrylic acid, polyvinyl alcohol.
Organic solvent in step b be in benzene, fluorobenzene, 1,2-ethylene dichloride one or more.
The present invention has the following advantages:
1. suitability is strong.Present method is urged mainly for the preparation of at biomedical diagnostic, microelectronics, chemistry
The polystyrene type foam microshell that the aspects such as change, high-energy physics experiment and Colloidal crystals template are widely used.
2. technique is simple, and process is easily controlled, with low cost, is easy to realize.With the synthesis preparation method ratio of existing polystyrene type foam microshell, the method, by introducing pore-creating agent and ultrasonic disperse generation microvesicle in oil-phase solution, is prepared porous material, is not needed complicated chemical reaction and loaded down with trivial details operation.
3. size tunable, narrow distribution range.The method for polymer microballoon technology, by regulating three-phase flow velocity, can control the size of Composite Milk grain based on microfluidic control, thus controls the geometrical dimension of ultimate aim microballoon, realizes size tunable and produces.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram in polystyrene type foam microshell cross section.
Embodiment
Below by embodiment, the present invention is specifically described.It is important to point out that following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to foregoing invention content to the present invention.
embodiment 1
Polystyrene, hexane and benzene are pressed 4.0:1.0:96.0 massfraction and configures oil-phase solution; Polyoxyethylene and water are pressed 0.01:99.9 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 1 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of the corresponding micro-injection pump of aqueous phase, oil phase and outer aqueous phase is 1.5ml/h, 3.0 ml/h and 200.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 20
oc, speed of rotation 25 rpm; After solidification about 96 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, with distilled water flushing, then microballoon is collected in sample bottle by microballoon, then uses distilled water and washes of absolute alcohol three times respectively, puts into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 330 μm-345 μm.
embodiment 2
Polystyrene, dodecane and fluorobenzene are pressed 15.0:5.0:90.0 massfraction and configures oil-phase solution; Polyacrylic acid and water are pressed 1.0:99.0 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 5 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of the corresponding micro-injection pump of aqueous phase, oil phase and outer aqueous phase is 1.0 ml/h, 4.0 ml/h and 400.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 45
oc, speed of rotation 45 rpm; After solidification about 72 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 690 μm-710 μm.
embodiment 3
Polystyrene, n-Hexadecane and 1,2-ethylene dichloride are pressed 25.0:10.0:65.0 massfraction and configures oil-phase solution; Polyvinyl alcohol and water are pressed 4.0:96.0 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 10 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of the corresponding micro-injection pump of aqueous phase, oil phase and outer aqueous phase is 2.0 ml/h, 6.0 ml/h and 800.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 65
oc, speed of rotation 65 rpm; After solidification about 48 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 845 μm-870 μm.
embodiment 4
Perduterated polystyrene, hexane and fluorobenzene are pressed 25.0:10.0:60.0 massfraction and configures oil-phase solution; Polyoxyethylene and water are pressed 0.01:99.9 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 10 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of aqueous phase, oil phase and outer corresponding micro-injection pump is 2.0 ml/h, 6.0 ml/h and 800.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 65
oc, speed of rotation 65 rpm; After solidification about 48 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 1010 μm-1030 μm.
embodiment 5
Perduterated polystyrene, dodecane and benzene are pressed 4.0:2.0:94.0 massfraction and configures oil-phase solution; Polyacrylic acid and water are pressed 0.04:99.6 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 4 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of the corresponding micro-injection pump of aqueous phase, oil phase and outer aqueous phase is 1.0 ml/h, 2.0 ml/h and 300.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 25
oc, speed of rotation 65 rpm; After solidification about 96 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 400 μm-420 μm.
embodiment 6
Perduterated polystyrene, n-Hexadecane and 1,2-ethylene dichloride are pressed 10.0:1.0:89.0 massfraction and configures oil-phase solution; Polyvinyl alcohol and water are pressed 4.0:96.0 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 6 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of the corresponding micro-injection pump of aqueous phase, oil phase and outer aqueous phase is 3.0 ml/h, 7.0 ml/h and 1000.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 55
oc, speed of rotation 35 rpm; After solidification about 96 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 870 μm-900 μm.
embodiment 7
Polystyrene, hexane and fluorobenzene are pressed 8.0:2.0:90.0 massfraction and configures oil-phase solution; Polyvinyl alcohol and water are pressed 2.0:98.0 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 3 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of the corresponding micro-injection pump of aqueous phase, oil phase and outer aqueous phase is 1.0 ml/h, 3.0 ml/h and 400.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 25
oc, speed of rotation 65 rpm; After solidification about 96 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 540 μm-565 μm.
embodiment 8
Perduterated polystyrene, n-Hexadecane and fluorobenzene are pressed 10.0:2.0:88.0 massfraction and configures oil-phase solution; Polyoxyethylene and water are pressed 1.0:99.0 massfraction and are configured the aqueous solution, filtering solution, and filtrate is as outer aqueous phase; By oil-phase solution ultrasonic 5 min before newborn grain preparation configured; the outer aqueous phase solution of 3 ml distilled water, 3ml oil-phase solution and 50 ml is drawn respectively with syringe; syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump; In regulating respectively, the flow velocity of the corresponding micro-injection pump of aqueous phase, oil phase and outer aqueous phase is 2.0 ml/h, 6.0 ml/h and 700.0 ml/h, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase; Collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 35
oc, speed of rotation 45 rpm; After solidification about 96 h, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains the polystyrene type hollow foam microballoon that particle diameter is 960 μm-990 μm.
Claims (6)
1. a preparation method for polystyrene type foam microshell, comprises the following steps:
A. polystyrenic polymer and pore-creating agent are dissolved in organic solvent, as oil phase;
B. newborn grain stablizer is dissolved in distilled water, filter, filtrate is as outer aqueous phase;
C. before newborn grain preparation, oil-phase solution is ultrasonic, a certain amount of distilled water, oil-phase solution and outer aqueous phase solution is drawn respectively with syringe, syringe is connected with aqueous phase, oil phase and outer aqueous phase pipeline in newborn grain producer respectively, and is fixed on corresponding micro-injection pump;
D. regulate the flow velocity of micro-injection pump, respectively distilled water, oil phase and outer aqueous phase are injected aqueous phase in newborn grain producer, oil phase and outer aqueous phase pipeline, prepare the Composite Milk grain of the coated distilled water of oil phase;
E. collect Composite Milk grain in the revolving bottle that outer aqueous phase is housed, and be arranged on the turning axle of Rotary Evaporators by revolving bottle, water-bath temperature control solidifies, temperature 20
oc ~ 65
oc, speed of rotation 25 rpm ~ 65 rpm, set time 48 h ~ 96 h;
F. after solidification terminates, pour the outer aqueous phase solution containing polystyrene type foam microshell into sizing screen, use distilled water flushing microballoon, then microballoon is collected in sample bottle, then use distilled water and washes of absolute alcohol three times respectively, put into baking oven, 45
oc is dry, obtains polystyrene type hollow foam microballoon.
2. the preparation method of polystyrene type foam microshell according to claim 1, is characterized in that: the mass percent in oil phase of the polystyrenic polymer in step a is 4.0% ~ 25.0%; Pore-creating agent mass percent in oil phase is 1.0% ~ 10%; Newborn grain stablizer in step b outside in aqueous phase mass percent be 0.01% ~ 4.0%.
3. the preparation method of polystyrene type foam microshell according to claim 1, is characterized in that: in step a, polystyrenic polymer is polystyrene or perduterated polystyrene.
4. the preparation method of polystyrene type foam microshell according to claim 1, is characterized in that: in step a, pore-creating agent is the one in hexane, dodecane, n-Hexadecane.
5. the preparation method of polystyrene type foam microshell according to claim 1, is characterized in that: in step b, newborn grain stablizer comprises the one in polyoxyethylene, polyacrylic acid, polyvinyl alcohol.
6. the preparation method of polystyrene type foam microshell according to claim 1, is characterized in that: the organic solvent in step b be in benzene, fluorobenzene, 1,2-ethylene dichloride one or more.
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| CN105778146A (en) * | 2016-05-11 | 2016-07-20 | 中国工程物理研究院激光聚变研究中心 | Method for customizing diameter and wall thickness of hollow polystyrene microsphere |
| CN105778146B (en) * | 2016-05-11 | 2018-12-11 | 中国工程物理研究院激光聚变研究中心 | A kind of method of polystyrene type tiny balloon diameter and wall thickness customization |
| CN106040116B (en) * | 2016-07-05 | 2019-04-26 | 中国工程物理研究院激光聚变研究中心 | A method of preparing the high sphericity polymer hollow microsphere of major diameter |
| CN107325320A (en) * | 2017-07-21 | 2017-11-07 | 中国工程物理研究院激光聚变研究中心 | The method for avoiding polystyrene type tiny balloon drying process from ftractureing |
| CN107325320B (en) * | 2017-07-21 | 2020-03-24 | 中国工程物理研究院激光聚变研究中心 | Method for preventing polystyrene hollow microsphere from cracking in drying process |
| CN108499498A (en) * | 2018-03-09 | 2018-09-07 | 中国工程物理研究院激光聚变研究中心 | A method of preparing the micro- tiny balloon of polymer |
| CN108499498B (en) * | 2018-03-09 | 2020-06-30 | 中国工程物理研究院激光聚变研究中心 | Method for preparing polymer micro hollow microsphere |
| CN108889253A (en) * | 2018-06-05 | 2018-11-27 | 中国工程物理研究院激光聚变研究中心 | The preparation method of high surface finish polystyrene hollow microballoon |
| CN108889253B (en) * | 2018-06-05 | 2020-02-21 | 中国工程物理研究院激光聚变研究中心 | Preparation method of polystyrene hollow microsphere with high surface smoothness |
| CN109553785A (en) * | 2018-12-05 | 2019-04-02 | 哈尔滨工业大学（深圳） | A kind of microfluidic control for micron size polystyrene spheres method |
| CN114405422A (en) * | 2022-01-19 | 2022-04-29 | 中国工程物理研究院激光聚变研究中心 | Fluid shaping device and method for preparing large-diameter polymer microspheres |
| CN114405422B (en) * | 2022-01-19 | 2023-02-28 | 中国工程物理研究院激光聚变研究中心 | Fluid shaping device and method for preparing large-diameter polymer microspheres |
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